Ethanol → 2-Hydroxy-3-bromo-4-chloro-5-(1,1-dimethylethyl)benzaldehyde oxime

HRID 1710002노트

반응식

HRID 1710002 반응식
[OH:1][C:2]1[C:9]([Br:10])=[C:8]([Cl:11])[C:7]([C:12]([CH3:15])([CH3:14])[CH3:13])=[CH:6][C:3]=1[CH:4]=O.Cl.[NH2:17][OH:18].C(O)C.C(=O)(O)[O-].[Na+]>O1CCCC1.O>[OH:1][C:2]1[C:9]([Br:10])=[C:8]([Cl:11])[C:7]([C:12]([CH3:15])([CH3:14])[CH3:13])=[CH:6][C:3]=1[CH:4]=[N:17][OH:18]

참가 물질

7

반응물 4

HCID 702EthanolHCID 443297Hydroxyamine hydrochlorideHCID 516892Sodium BicarbonateHCID 230354152-Hydroxy-3-bromo-4-chloro-5-(1,1-dimethylethyl)benzaldehyde

생성물 1

HCID 1364045082-Hydroxy-3-bromo-4-chloro-5-(1,1-dimethylethyl)benzaldehyde oxime수율 85%

시약·촉매·용매 2

HCID 962Water용매2회HCID 8028Tetrahydrofuran용매

실험 절차

A mixture of 2.25 g (7.72 mmol) of 2-hydroxy-3-bromo-4-chloro-5-(1,1-dimethylethyl)benzaldehyde and 0.59 g (8.49 mmol) of hydroxylamine hydrochloride in 15 ml of 1:1:1 tetrahydrofuran:ethanol:water was cooled in an ice-water bath. Sodium bicarbonate (0.78 g, 9.26 mmol) was added in small portions over 15 minutes. After stirring overnight at ambient temperature, water (25 ml) was added and the solid was filtered and dried. There was obtained 2.00 g (6.52 mmol, 85%) of 2-hydroxy-3-bromo-4-chloro-5-(1,1-dimethylethyl)benzaldehyde oxime as a white solid after crystallization from cyclohexane mp 175°-177° C.

후처리

  1. filtrationthe solid was filtered
  2. customdried

출처 및 근거

ORD 기록
ord-0a0e0be3a83846a4a00ecb16d29a45ac
출처 데이터셋
uspto-grants-1990_08
특허 번호
US04952583

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